反应详情

N-(6-methoxypyridin-3-yl)-3-(2-methyl-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-yl)-5-(4-(methylsulfonyl)benzyl)pyridin-2-amine (94.5 mg, 0.161 mmol) was suspended in a mixture of 2 M aqueous HCl (2.0 mL) and water (6 mL). The mixture was heated at reflux for 1 h and then allowed to cool and stand at room temperature over the weekend. The resulting solid was collected by filtration, washed with water, and dried to give N-(6-methoxypyridin-3-yl)-3-(2-methyl-9H-purin-6-yl)-5-(4-(methylsulfonyl)benzyl)pyridin-2-amine hydrochloride (75.7 mg, 0.141 mmol, 87% yield) as a yellow solid. 1H NMR (400 MHz, d6-DMSO) δ 12.50 (br. s., 1H); 9.66 (br. s., 1H); 8.60 (s, 1H); 8.52 (d, J=2.54 Hz, 1H); 8.26 (d, J=1.96 Hz, 1H); 8.16 (dd, J=8.80, 2.74 Hz, 1H); 7.87 (d, J=8.22 Hz, 2H); 7.57 (d, J=8.22 Hz, 2H); 6.85 (d, J=8.80 Hz, 1H); 4.13 (s, 2H); 3.85 (s, 3H); 3.17 (s, 3H); 2.84 (s, 3H). m/z (ESI, +ve ion) 502.0 (M+H)+.

1. temperatureThe mixture was heated
2. temperatureat reflux for 1 h
3. temperatureto cool
4. customstand at room temperature over the weekend
5. filtrationThe resulting solid was collected by filtration
6. washwashed with water
7. customdried